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🧲 Structure Identification · Method

NMR Spectroscopy

Map the C–H skeleton to identify structure
🎯 Difficulty ★★☆ Medium Duration About 30 min–1 h 🎯 Use Record ¹H and ¹³C NMR to confirm structure, purity, and stereochemistry.
📖 Principle
Nuclei absorb specific frequencies that reveal their local chemical environment.
Below are 4 steps. Open each to see how to do it and add products to your shared list.

📋 Workflow

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1

Dissolve the sample

10 min
Dissolve 5–15 mg in 0.5 mL deuterated solvent, transfer to an NMR tube.
💡 Tip Clear, particle-free solutions give cleaner spectra
⚠️ Caution Deuterated solvents absorb H₂O; keep sealed
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2

Load and shim

10 min
Load the tube, lock and shim until peaks are symmetric and sharp.
💡 Tip Good shimming narrows lines and improves integration
⚠️ Caution Gas bubbles disturb shimming
🧪 Materials for this step (click to shop by spec/brand)
3

Acquire spectra

15–30 min
Set the ¹H pulse sequence, scans, and spectral width, acquire; then ¹³C and needed 2D.
💡 Tip Run DEPT/HSQC when needed for assignment
⚠️ Caution Too few scans give poor ¹³C S/N
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4

Analyze and assign

20 min
Process in software, integrate and assign peaks, compare with the expected structure.
💡 Tip Multiplicities and J values reveal substitution patterns
⚠️ Caution Don't mistake residual solvent peaks for product
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⚠️ 5 Common Beginner Mistakes

  • Too little sample, ¹³C shows nothing
  • Water/solvent peak obscures target signal
  • Misassigning residual solvent as product
  • Poor shimming broadens lines and skews integration
  • Paramagnetic impurity distorts peaks

❓ FAQ

+Which deuterated solvent?
CDCl₃ for routine; DMSO-d₆ or D₂O for polar samples.
+Assess purity by NMR?
Check for unexpected extra peaks and integral ratios.
+When to run 2D?
When assignment is ambiguous or overlapping—COSY/HSQC/HMBC.

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Data authenticity: Product categories from JW Supply Chain standard taxonomy; method→step→product connected. Last updated: 2026-08-23 · v3.0